分散液液微萃取/气相色谱-质谱法同时测定烟用添加剂中8种烷基苯类香味有害物

Simultaneous Determination of Alkenylbenzenes and Other Flavor-related Compounds in Tobacco Additives by Dispersive Liquid-Liquid Micro-extraction and GC-MS

建立了超声溶剂提取和分散液液微萃取(DLLME)相结合的提取、净化前处理技术,采用气相色谱-质谱法分析了烟用添加剂中的黄樟素、侧柏酮、龙蒿脑、胡薄荷酮、甲基丁香酚、香豆素、6-甲基香豆素和7-甲氧基香豆素8种烷基苯类香味有害物。对分散液液微萃取溶剂及其体积、分散剂及其体积、萃取时间等条件进行了优化。在最佳实验条件下,8种有害物的线性范围为0.4～928μg/L(r2≥0.998 9),检出限为0.04～0.24μg/L,定量下限为0.13～0.80μg/L,富集倍数为140～208倍,方法的加标回收率为90%～100%,相对标准偏差为2.4%～6.7%。与行业推荐的测定方法相比,该方法具有灵敏度高、富集效果好、回收率高等优点。

A new ultrasonic-assisted extraction followed by dispersive liquid -liquid micro-extraction （DLLME） and GC - MS analysis method was developed for the simultaneous determination of eight alkenylbenzenes and other flavor-related compounds including safrole, coumarin, 6-methylcoumarin, 7-metheoxycomnarin, estragole, methyleugenol, pulegone and thujone in tobacco additives. The different parameters affecting the whole process such as the type and volume of extraction and dis- perser solvents, the salt addition and the extraction time were studied. Under the optimum condi- tions, the enrichment factors（EF） ranged from 140 to 208. The linear relationships of eight alkenyl- benzenes and other flavor-related compounds were obtained in the range of 0.4 -928 μg/L, with cor- relation coefficients （ r^2 ） over O. 998 9. The limits of detection （LOD） and the limits of quantitation （LOQ） were in the ranges of 0.04 -0.24 μg/L and 0. 13 -0. 80 μg/L, respectively. The average recoveries were in the range of 90% - 100% with relative standard deviatigns （RSDs） of 2.4% - 6.7% . The method was successfully applied in the analysis of real tobacco flavor additive samples. Compared with the industry recommended standard method, lower concentrations of detection were a- chieved due to the high enrichment power of DLLME. Therefore, this method shows tremendous po- tential in trace analysis of alkenylbeuzenes and other flavor-related compounds in real samples.